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[纳米多孔二氧化硅薄膜的制备及红外光谱分析]

[Preparation and infrared spectral analysis of nanoporous silica thin film].

作者信息

Wang Juan, Zhang Chang-rui, Feng Jian, Yang Da-xiang

机构信息

Key Lab of Advanced Ceramic Fibers and Composites, College of Aerospace and Material Engineering, National University of Defense Technology, Changsha 410073, China.

出版信息

Guang Pu Xue Yu Guang Pu Fen Xi. 2005 Jul;25(7):1045-8.

Abstract

Crack-free homogeneous nanoporous silica films on silicon wafer have been synthesized via supercritical drying of wet gel films obtained by spin-coating the polymeric silica sol, which was prepared using sol-gel method with tetraethoxysilane (TEOS) as precursor. The film is amorphous and nanoporous, and three-dimensional network, cross-linked by the primary particles whose sizes distribute between 10-20 nm showed respectively by XRD and SEM micrograph. The structure of the nanoporous SiO2 thin film was studied by FTIR spectra. The SiO2 thin film was composed of Si-O-Si and Si-OR, and was hydrophobic. The film contained Si-OH and became hydrophilic after being heat-treated at 250 degrees C or above in air. The heat-treated SiO2 thin film becomes hydrophobic by reacting with trimethylchlorosilane(TMCS). The TMCS-modified SiO2 thin film remains hydrophobic and can keep its nanoporous structure at a temperature lower than 450 degrees C in nitrogen.

摘要

通过对采用溶胶 - 凝胶法以四乙氧基硅烷(TEOS)为前驱体制备的聚合物硅溶胶进行旋涂得到的湿凝胶膜进行超临界干燥,在硅片上合成了无裂纹的均匀纳米多孔二氧化硅薄膜。该薄膜为非晶态且具有纳米多孔结构,通过X射线衍射(XRD)和扫描电子显微镜(SEM)显微照片分别显示其由尺寸分布在10 - 20纳米之间的初级粒子交联形成三维网络结构。利用傅里叶变换红外光谱(FTIR)对纳米多孔二氧化硅薄膜的结构进行了研究。该二氧化硅薄膜由Si - O - Si和Si - OR组成,具有疏水性。薄膜含有Si - OH,在空气中250℃及以上进行热处理后变为亲水性。经过热处理的二氧化硅薄膜通过与三甲基氯硅烷(TMCS)反应又变为疏水性。TMCS改性的二氧化硅薄膜保持疏水性,并且在氮气中低于450℃的温度下能够保持其纳米多孔结构。

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